CN113913908B - Preparation method of thick nickel-plated profiling anode for inner profile of saddle rotary body - Google Patents

Preparation method of thick nickel-plated profiling anode for inner profile of saddle rotary body Download PDF

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Publication number
CN113913908B
CN113913908B CN202111005135.3A CN202111005135A CN113913908B CN 113913908 B CN113913908 B CN 113913908B CN 202111005135 A CN202111005135 A CN 202111005135A CN 113913908 B CN113913908 B CN 113913908B
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nickel
anode
casting
treatment
adopting
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CN113913908A (en
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刘兴斌
翟绘丰
杨战争
权琳琳
姚鹏
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Xian Aerospace Engine Co Ltd
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Xian Aerospace Engine Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C25D17/12—Shape or form
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention relates to a preparation method of a profiling anode with thick nickel plated on the inner profile of a saddle rotary body, which comprises the manufacturing process and method of the anode. When the inner surface of the workpiece is plated, in order to ensure the area ratio of the anode to the plated workpiece, the surface area of the inner anode needs to be increased as much as possible, and the anode is generally manufactured by adopting a scheme of welding after metal plate processing. The thickness of the nickel plate cannot be larger than 3mm during metal plate processing, and the obtained anode is difficult to meet the long-time nickel plating dissolution requirement. The thickness of the nickel anode is processed to a required value by adopting a proper treatment scheme through a nickel casting method, and the prepared anode can meet the requirement of long-time nickel plating.

Description

Preparation method of thick nickel-plated profiling anode for inner profile of saddle rotary body
Technical Field
The invention belongs to the technical field of electrochemical surface treatment, and particularly relates to a method for preparing a thick nickel coating on the inner surface of a workpiece with a rotary inner profile structure, wherein a profiling inner anode is used for obtaining a coating with better surface quality, uniformity and binding force. The anode blank is manufactured by adopting a scheme of welding after metal plate processing, and then the thickness of the anode is increased by electroforming nickel so as to meet the requirement of long-time nickel plating.
Background
When a certain component in the novel liquid rocket engine works, high-temperature oxygen-enriched fuel gas passes through the inner cavity, and thick nickel plating protection is adopted for protecting the inner wall of the component. The inner wall of the assembly is of a rotary saddle body structure, and a profiling inner anode is needed during electroplating in order to ensure the surface quality, binding force and uniformity of a plating layer.
In the electrochemical field, an internal anode and an auxiliary anode are commonly used, but the area ratio of the anode to the cathode is small when the internal surface is electroplated, and passivation phenomenon is easy to occur due to insufficient anode area. In order to enlarge the area of the inner anode as much as possible, a scheme of metal plate processing, welding and forming is adopted to manufacture the inner anode. Because the nickel plate hardness is great, the nickel plate that thickness is greater than 3mm is difficult to process when panel beating, and the positive pole of 3mm thick nickel plate preparation is difficult to satisfy long-time nickel plating dissolution demand. The anode can have the phenomena of partial dissolution loss, welding seam detachment and the like in the plating process.
Disclosure of Invention
The invention solves the technical problems that: overcomes the defects of the prior art and provides a preparation method of a profile-plated thick nickel profiling anode in a saddle rotary body.
The solution of the invention is as follows: the preparation method of the profile thick nickel plating profiling anode in the saddle rotary body comprises the following steps:
s1, processing an anode blank by using a nickel plate with the thickness of 3mm or less, and plating the anode to the required thickness by a nickel casting method; the nickel casting method comprises the following steps:
s2, carrying out oil removal treatment on the surface of the anode blank, and then carrying out acid washing to remove an oxide film on the surface of the anode blank;
s3, performing activation treatment on the anode blank after the treatment;
s4, adopting a cast nickel solution, wherein the temperature is 45-60 ℃ and the current density is 1.5-3.5A/dm 2 Carrying out nickel casting treatment by adopting a mode of cathode movement or compressed gas stirring, wherein the single nickel casting time is 8-10h;
and S5, trimming the plating layer obtained after the cast nickel treatment, and returning to S3 after acid washing again if the trimmed plating layer does not reach the required thickness until the thickness meets the requirement.
Preferably, the cast nickel treatment in S4 is carried out stepwise, first at 1.5-2A/dm 2 Selecting current density in a range, and casting nickel for 1-2 hours for a single time; then at 2-3A/dm 2 Selecting current density in a range, and casting nickel for 3-4 hours for a single time; finally at 3-3.5A/dm 2 And selecting current density in a range, and casting nickel for 4 hours for a single time.
Preferably, the degreasing treatment is performed by first degreasing with a solvent or a chemical, and then performing an electrochemical treatment.
Preferably, the electrochemical treatment adopts cathodic electrochemical degreasing treatment and adopts 60 composed of sodium carbonate, sodium phosphate and sodium silicateAlkaline solution at the temperature of between DEG C and 90 ℃ for 3 to 5 minutes and current density of between 1 and 5A/dm 2 。
Preferably, the chemical degreasing adopts alkaline solution composed of sodium hydroxide, sodium carbonate, sodium phosphate and sodium silicate at 60-90 ℃ for 15-30min.
Preferably, the acid washing in S2 employs:
150-250g/L HCl; or H 2 SO 4 60-100g/L、HNO 3 50-100g/L, HF-50 g/L of mixed acid solution; or the HCl and the mixed acid solution are combined for acid washing.
Preferably, the activation treatment is carried out by using 30-50g/L sulfuric acid or hydrochloric acid solution for 1-3min.
Preferably, 150-250g/L HCl is used for repeated acid washing in S5.
Preferably, the nickel casting is repeated no more than 6 times.
Compared with the prior art, the invention has the beneficial effects that:
(1) In order to avoid the phenomena of partial dissolution loss, weld joint detachment and the like of a conventional sheet metal processing nickel anode in the long-time plating process, the invention prepares nickel with a certain thickness on the surface of the nickel anode by a nickel casting method so as to meet the use requirement of long-time plating. When nickel is cast, a proper treatment method and a proper procedure are adopted, so that the nickel layer has a certain thickness, the purity is not lower than that of electrolytic nickel, and the binding force is good.
(2) The current density is 1.5-3.5A/dm 2 Better deposition speed and coating quality can be obtained. After 8-10 hours of nickel casting, trimming is carried out, so that the nickel layer can be prevented from being too rough to be effectively deposited. If the nickel layer is too rough, nickel casting is continued, round point-shaped, columnar or dendritic knots are generated on the surface of the nickel layer, and most of the obtained nickel layer is deposited on the knots, so that the nickel layer does not contribute to the size increase of the anode.
(3) The method for sectional nickel casting can slow down the roughening speed of the nickel layer, and has better economic benefit (better plating thickness and quality can be obtained with less resource consumption) under the condition of 8-10 hours of sectional nickel casting through practical production verification conclusion.
Detailed Description
The invention is further illustrated below with reference to examples.
Anode processing flow: cutting a nickel plate (with the thickness of 3mm or less) according to the design size, welding sheet metal processing parts into an anode blank, and casting nickel on the surface of the blank to the required thickness.
The nickel anode blank cast nickel processing flow comprises the following steps: deoiling, electrochemical deoiling, pickling, activating, nickel casting, trimming the profile and repeatedly nickel casting to the thickness to meet the requirements.
The nickel anode blank body nickel casting comprises the following specific steps:
(1) Deoiling
According to the oil stain condition of the surface of the anode blank, one of solvent oil removal and chemical oil removal is selected, and the oil removal can be performed in a combined mode.
Solvents commonly used for solvent degreasing are: gasoline, alcohol or other organic solvents.
The chemical degreasing adopts an alkaline solution which consists of sodium hydroxide, sodium carbonate, sodium phosphate and sodium silicate and is at 60-90 ℃ for 15-30min, and the oil stain is removed completely.
(2) Electrochemical treatment
An alkaline solution composed of sodium carbonate, sodium phosphate and sodium silicate at 60-90 ℃ is adopted, and in order to avoid passivation of nickel plates, cathode electrochemical degreasing is generally adopted for 3-5min and current density is 1-5A/dm 2 。
(3) Acid washing
Pickling with HCl 150-250g/L for 10-20min; or adopt H 2 SO 4 60-100g/L、HNO 3 50-100g/L, HF-50 g/L of the mixed acid solution, and pickling for 5-10min. The pickling time can be prolonged according to the removal condition of the oxide film on the surface of the anode blank or the combination of the two solutions can be adopted.
(4) Activation of
The preparation method is carried out by adopting 30-50g/L sulfuric acid or hydrochloric acid solution for 1-3min.
(5) Cast nickel
Adopting cast nickel solution with temperature of 45-60deg.C and current density of 1.5-3.5A/dm 2 By taking the following steps ofThe cathode moves or is stirred by introducing compressed gas, and the single nickel casting time is preferably 8-10 hours.
The invention provides a preferred treatment mode, firstly [1.5,2]A/dm 2 Selecting current density in a range, and casting nickel for 1-2 hours for a single time; then at (2, 3) A/dm 2 Selecting current density in a range, and casting nickel for 3-4 hours for a single time; finally at [3,3.5 ]]A/dm 2 And selecting current density in a range, and casting nickel for 4 hours for a single time.
(6) Trimming profiles
The plating layer is generally trimmed by a mechanical method, and the knots, burrs and excessive plating layers deposited on the surface of the plating layer are removed so as to meet the final design profile of the anode.
(7) Repeatedly cast nickel
After finishing the profile, the nickel can be cast again according to the steps, and the pickling process is carried out by adopting hydrochloric acid solution when the nickel casting is repeated, wherein the repeated times are based on the fact that the thickness of the anode meets the design size. The nickel layer with the thickness of more than 8mm can be obtained by repeatedly casting nickel for a plurality of times.
Example 1
The anode blank formed by welding metal plates is cast with nickel according to the method, and after chemical degreasing and cathode electrochemical degreasing, H is used for 2 SO 4 、HNO 3 Pickling with HF mixed acid solution for 5min, activating, and casting nickel solution at 45-60 deg.c at 2A/dm 2 Nickel casting for 1h; then at 2.5A/dm 2 Nickel casting for 4h; finally at 3A/dm 2 The current density of the alloy is cast for 4 hours, the molded surface is polished and trimmed after the nickel casting, and the process is repeated twice according to the flow procedure. The nickel layer with the thickness of 3-4mm can be obtained, the nickel layer has good bonding force with the anode blank body, no cracking and peeling phenomena are caused, and the nickel layer does not fall off in the use process. The anode can work continuously for 12-15h when being used for plating a workpiece.
Example 2
The anode blank formed by welding metal plates is cast with nickel according to the method, and after chemical degreasing and cathode electrochemical degreasing, H is used for 2 SO 4 、HNO 3 Pickling with HF mixed acid solution for 10min, activating, and casting nickel solution at 45-60 deg.c at 1.5A/dm 2 Nickel casting for 1.5h; then at 2.3A/dm 2 Nickel casting for 3h; finally at 3.5A/dm 2 The current density of the alloy is cast for 4 hours, the molded surface is polished and trimmed after the nickel casting, and the process is repeated three times according to the flow procedure. The nickel layer with the thickness of 5-6mm can be obtained, the nickel layer has good bonding force with the anode blank body, no cracking and peeling phenomena are caused, and the nickel layer does not fall off in the use process. The anode can work continuously for 15-20h when being used for plating a workpiece.
Example 3
The anode blank formed by welding metal plates is cast with nickel according to the method, after chemical degreasing and cathodic electrochemical degreasing, the anode blank is pickled for 10min by HCl solution, and after activation, the anode blank is cast with nickel solution at 45-60 ℃ at 2A/dm 2 Nickel casting for 2h; then at 2.8A/dm 2 Nickel casting for 4h; finally at 3.5A/dm 2 The current density of the alloy is cast for 4 hours, the molded surface is polished and trimmed after the nickel casting, and the process is repeated three times according to the flow procedure. The nickel layer with the thickness of 6-7mm can be obtained, the nickel layer has good bonding force with the anode blank body, no cracking and peeling phenomena are caused, and the nickel layer does not fall off in the use process. The anode can continuously work for 20-25h when being used for plating a workpiece.
Example 4
The anode blank formed by welding metal plates is cast with nickel according to the method, after chemical degreasing and cathodic electrochemical degreasing, the anode blank is pickled with HCl solution for 20min, and after activation, the anode blank is cast with nickel solution at 45-60 ℃ at 1.5A/dm 2 Nickel casting for 1h; then at 2.5A/dm 2 Nickel casting for 3h; finally at 3A/dm 2 The nickel is cast for 4 hours, the molded surface is polished and trimmed after the nickel is cast, and the process is repeated four times according to the flow procedure. The nickel layer with the thickness of 6-7mm can be obtained, the nickel layer has good bonding force with the anode blank body, no cracking and peeling phenomena are caused, and the nickel layer does not fall off in the use process. The anode can continuously work for 20-25h when being used for plating a workpiece.
Example 5
The anode blank formed by welding metal plates is cast with nickel according to the method, after chemical degreasing and cathodic electrochemical degreasing, the anode blank is pickled for 10min by HCl solution, and after activation, the anode blank is cast with nickel solution at 45-60 ℃ at 2A/dm 2 Nickel casting for 1.5h; then at 2.8A/dm 2 Nickel casting for 4h; most preferably, the first to fourthThereafter, the reaction was carried out at 3.5A/dm 2 The nickel is cast for 4 hours, the molded surface is polished and trimmed after the nickel is cast, and the process is repeated four times according to the flow procedure. The nickel layer with the thickness of 7-9mm can be obtained, the nickel layer has good bonding force with the anode blank body, no cracking and peeling phenomena are caused, and the nickel layer does not fall off in the use process. The anode can work continuously for 25-32h when being used for plating a workpiece.
Although the present invention has been described in terms of the preferred embodiments, it is not intended to be limited to the embodiments, and any person skilled in the art can make any possible variations and modifications to the technical solution of the present invention by using the methods and technical matters disclosed above without departing from the spirit and scope of the present invention, so any simple modifications, equivalent variations and modifications to the embodiments described above according to the technical matters of the present invention are within the scope of the technical matters of the present invention.
The invention is not described in detail in part as being common general knowledge to a person skilled in the art.

Claims (6)

1. The preparation method of the profile thick nickel plating profiling anode in the saddle rotary body is characterized by comprising the following steps:
s1, processing an anode blank by using a nickel plate with the thickness of 3mm or less, and plating the anode to the required thickness by a nickel casting method; adopting a scheme of welding after metal plate processing to manufacture an anode blank, and then enlarging the thickness of the anode by electroforming nickel so as to meet the long-time nickel plating requirement;
the nickel casting method comprises the following steps:
s2, carrying out oil removal treatment on the surface of the anode blank, and then carrying out acid washing to remove an oxide film on the surface of the anode blank; the pickling in S2 adopts:
150-250g/L HCl; or H 2 SO 4 60-100g/L、HNO 3 50-100g/L, HF-50 g/L of mixed acid solution; or the HCl and the mixed acid solution are combined for acid washing;
s3, performing activation treatment on the anode blank after the treatment;
s4, adopting a cast nickel solution at 45-60 DEG CThe current density is 1.5-3.5A/dm 2 Carrying out nickel casting treatment by adopting a mode of cathode movement or compressed gas stirring, wherein the single nickel casting time is 8-10h; in S4, the nickel casting treatment is carried out in a sectional manner, and firstly, the nickel casting treatment is carried out at 1.5-2A/dm 2 Selecting current density in a range, and casting nickel for 1-2 hours for a single time; then at 2-3A/dm 2 Selecting current density in a range, and casting nickel for 3-4 hours for a single time; finally at 3-3.5A/dm 2 Selecting current density in a range, and casting nickel for 4 hours for a single time;
s5, trimming the plating layer obtained after the cast nickel treatment, and returning to S3 after pickling again if the trimmed plating layer does not reach the required thickness until the thickness meets the requirement;
the activation treatment is carried out by adopting 30-50g/L sulfuric acid or hydrochloric acid solution for 1-3min.
2. The method according to claim 1, characterized in that: the degreasing treatment firstly adopts solvent and/or chemical degreasing, and then carries out electrochemical treatment.
3. The method according to claim 2, characterized in that: the electrochemical treatment adopts cathode electrochemical degreasing treatment, adopts alkaline solution composed of sodium carbonate, sodium phosphate and sodium silicate at 60-90 ℃ for 3-5min and current density of 1-5A/dm 2 。
4. The method according to claim 2, characterized in that: the chemical degreasing adopts an alkaline solution which consists of sodium hydroxide, sodium carbonate, sodium phosphate and sodium silicate and is at 60-90 ℃ for 15-30min.
5. The method according to claim 1, characterized in that: and S5, repeatedly pickling by adopting 150-250g/L HCl.
6. The method according to claim 1, characterized in that: the number of times of repeated nickel casting is not more than 6.
CN202111005135.3A 2021-08-30 2021-08-30 Preparation method of thick nickel-plated profiling anode for inner profile of saddle rotary body Active CN113913908B (en)

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CN101397686B (en) * 2007-09-27 2010-10-13 宝山钢铁股份有限公司 Method for preparing nickel base alloy surface composite plating
CN101353807A (en) * 2008-09-22 2009-01-28 北京科技大学 Method for producing nickel shaped charge liner using nickel sulfate electroforming solution
CN104233420A (en) * 2013-06-14 2014-12-24 无锡市森信精密机械厂 Method for directly electroplating high-binding-force nickel layer on surface of aluminum or aluminum alloy
CN103556192B (en) * 2013-10-09 2016-03-30 北京航空航天大学 A kind of bidirectional pulse power supply that adopts prepares the method with strong mechanical performance electroforming nickel dam
CN108221006A (en) * 2018-02-11 2018-06-29 常德金德新材料科技股份有限公司 A kind of efficient method for preparing nickel plate

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